Raw material collection system, substrate processing apparatus, raw material collection method, and semiconductor device manufacturing method

Abstract

The present invention is provided with: an exhaust pipe for discharging a process gas containing a metal-containing raw material from a process chamber, the exhaust pipe having a first exhaust line; a collection unit which is provided in the first exhaust line and collects a metal-containing raw material from the process gas; and a heating unit that heats the collection unit in accordance with the viscosity of the metal-containing raw material.

Description

Technical Field

[0001] The present disclosure relates to a raw material collection system, a substrate processing apparatus, a raw material collection method, and a method for manufacturing a semiconductor device. Background Art

[0002] Patent Document 1 discloses the installation of a collector in a substrate processing apparatus for recovering and reusing Ru raw material (Ru(EtCp)2), which does not contribute to film formation on the substrate. Patent Document 2 also discloses the installation of a collector in a semiconductor manufacturing apparatus for recovering Ta raw material (Ta(OC2H5)5). Furthermore, Patent Document 3 discloses the installation of a bypass pipe that bypasses the collector in a substrate processing apparatus.

[0003] Prior art literature

[0004] Patent Literature

[0005] Patent Document 1: Japanese Patent Application Laid-Open No. 2006-2174

[0006] Patent Document 2: Japanese Patent Application Laid-Open No. 2002-110660

[0007] Patent Document 3: Japanese Patent Application Laid-Open No. 2011-35191 Summary of the Invention

[0008] Problems to be solved by the invention

[0009] In recent years, the use of liquids whose viscosity changes with temperature, which are difficult to handle, as raw materials for film formation has increased. In addition, from the perspectives of cost and resource conservation, it is desired to recycle raw materials containing precious metals.

[0010] The present disclosure provides a technology capable of recovering a raw material whose viscosity changes with temperature from gas exhausted from a substrate processing chamber.

[0011] Means for solving problems

[0012] According to one embodiment of the present disclosure, a technology is provided, comprising: an exhaust pipe that exhausts a process gas containing a metal-containing raw material from a process chamber and has a first exhaust line; a collecting portion that is disposed in the first exhaust line and captures the metal-containing raw material from the process gas; and a heating portion that heats the collecting portion according to the viscosity of the metal-containing raw material.

[0013] Effects of the Invention

[0014] According to the present disclosure, a raw material whose viscosity changes depending on temperature can be recovered from gas exhausted from a substrate processing chamber. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] Figure 1 This is a schematic longitudinal sectional view of a vertical processing furnace of a substrate processing apparatus according to one embodiment of the present disclosure.

[0016] Figure 2 This is a diagram showing a state in which the treated gas flows through the first exhaust line and the collection unit to be detoxified in the raw material capture system.

[0017] Figure 3 This is a front view showing the collecting section and the storage section.

[0018] Figure 4A It is a longitudinal sectional view of the collecting part.

[0019] Figure 4B yes Figure 4A HH cross-sectional view in.

[0020] Figure 5 It is a cross-sectional view showing the guide portion.

[0021] Figure 6 This is a schematic configuration diagram of a controller of a substrate processing apparatus according to one embodiment of the present disclosure, and is a diagram showing a control system of the controller using a block diagram.

[0022] Figure 7 It is a diagram showing a modified example of the substrate processing step in one embodiment of the present disclosure.

[0023] Figure 8 This is a diagram showing a state in which the treated gas in the raw material capture system flows through the second exhaust line to the detoxification process.

[0024] Figure 9 This is a diagram showing a state in which the processed gas flows through the first exhaust line and the collecting section toward the detoxification process in the raw material capture system of Modification 1. DETAILED DESCRIPTION

[0025] The present embodiment will be described below with reference to the accompanying drawings. The drawings used in the following description are schematic, and the dimensional relationships and proportions of the elements shown in the drawings may not necessarily correspond to reality. Furthermore, the dimensional relationships and proportions of the elements shown in the drawings may not necessarily be consistent across multiple drawings.

[0026] (1) Structure of substrate processing apparatus

[0027] The substrate processing apparatus 10 includes a processing furnace 202 provided with a heater 207 as a heating unit (heating mechanism, heating system). The heater 207 is cylindrical and is vertically mounted by being supported by a heater base (not shown) as a holding plate.

[0028] On the inner side of the heater 207, an outer tube 203 constituting a reaction vessel (processing vessel) is arranged concentrically with the heater 207. The outer tube 203 is made of a heat-resistant material such as quartz (SiO2) or silicon carbide (SiC), and is formed into a cylindrical shape with a closed upper end and an open lower end. Below the outer tube 203, a manifold (inlet flange) 209 is arranged concentrically with the outer tube 203. The manifold 209 is made of a metal such as stainless steel (SUS), and is formed into a cylindrical shape with an open upper end and a lower end. An O-ring 220a is provided as a sealing member between the upper end of the manifold 209 and the outer tube 203. The manifold 209 is supported by the heater base, whereby the outer tube 203 is mounted vertically.

[0029] Inside outer tube 203, inner tube 204, forming the reaction vessel, is disposed. Inner tube 204 is made of a heat-resistant material such as quartz (SiO2) or silicon carbide (SiC), and is cylindrical with a closed top and an open bottom. The outer tube 203, inner tube 204, and manifold 209 primarily constitute the processing vessel (reaction vessel). The processing chamber 201 is formed within the hollow portion of the processing vessel (inside inner tube 204).

[0030] The processing chamber 201 is configured to accommodate wafers 200 as substrates in a horizontal posture and arranged in multiple stages in the vertical direction via a boat 217 to be described later.

[0031] In the processing chamber 201, nozzles 410, 420, 430, and 440 are provided so as to penetrate the sidewall of the manifold 209 and the inner tube 204. The nozzles 410, 420, 430, and 440 are connected to the gas supply pipes 310, 320, 330, and 340, respectively. However, the processing furnace 202 of this embodiment is not limited to the above configuration.

[0032] Gas supply pipes 310, 320, 330, and 340 are connected to the integrated gas system 20. Nozzles 410, 420, 430, and 440 are connected to the front ends of the gas supply pipes 310, 320, 330, and 340, respectively. Nozzles 410, 420, 430, and 440 are L-shaped, with their horizontal portions extending through the sidewalls of the manifold 209 and the inner tube 204. The vertical portions of nozzles 410, 420, 430, and 440 are located within the channel-shaped (groove-shaped) preparatory chamber 201a. Within the preparatory chamber 201a, they extend upward (above the direction in which the wafers 200 are arranged) along the inner wall of the inner tube 204. The preparatory chamber 201a is formed to protrude radially outward from the inner tube 204 and extend vertically.

[0033] The nozzles 410, 420, 430, and 440 are arranged to extend from the lower area of the processing chamber 201 to the upper area of the processing chamber 201, and multiple gas supply holes 410a, 420a, 430a, and 440a are respectively provided at positions opposite the wafer 200. Thus, processing gas is supplied to the wafer 200 from the gas supply holes 410a, 420a, 430a, and 440a of the nozzles 410, 420, 430, and 440, respectively. Multiple gas supply holes 410a, 420a, 430a, and 440a are arranged from the bottom to the top of the inner tube 204, each having the same opening area and arranged at the same opening spacing. However, the gas supply holes 410a, 420a, 430a, and 440a are not limited to the above configuration. For example, the opening area may gradually increase from the bottom to the top of the inner tube 204. This makes it possible to make the flow rate of the gas supplied from the gas supply holes 410 a , 420 a , 430 a , and 440 a more uniform.

[0034] A plurality of gas supply holes 410a, 420a, 430a, and 440a of nozzles 410, 420, 430, and 440 are provided at heights extending from the bottom to the top of a wafer boat 217 (described later). Therefore, the process gas supplied into the processing chamber 201 from the gas supply holes 410a, 420a, 430a, and 440a of the nozzles 410, 420, 430, and 440 is supplied to the entire area of the wafers 200 accommodated, from the bottom to the top of the wafer boat 217. The nozzles 410, 420, 430, and 440 can be provided to extend from the bottom to the top of the processing chamber 201, but are preferably provided to extend to near the top of the wafer boat 217.

[0035] A metal-containing gas, which is a raw material gas containing a metal element, is supplied as a process gas from a gas supply pipe 310 through the integrated gas system 20 and the nozzle 410 into the process chamber 201 .

[0036] Reducing gas is supplied as a processing gas from the gas supply pipe 320 into the processing chamber 201 via the integrated gas system 20 and the nozzle 420 .

[0037] An oxygen-containing gas containing oxygen atoms (O) is supplied from the gas supply pipe 330 through the nozzle 430 into the processing chamber 201 as a processing gas.

[0038] A halogen-containing gas, which is a gas containing a halogen element, is supplied as a processing gas from the gas supply pipe 340 through the nozzle 440 into the processing chamber 201 .

[0039] Inert gases are supplied from the integrated gas system 20 into the processing chamber 201 through the nozzles 410 , 420 , 430 , and 440 , respectively.

[0040] As the inert gas, for example, rare gases such as nitrogen (N2) gas, argon (Ar) gas, helium (He) gas, neon (Ne) gas, and xenon (Xe) gas can be used. More than one of these gases can be used as the inert gas. This also applies to the other inert gases described later.

[0041] The process gas supply system primarily comprises gas supply pipes 310, 320, 330, 340 and nozzles 410, 420, 430, and 440. However, nozzles 410, 420, 430, and 440 may be considered the process gas supply system alone. The process gas supply system may also be simply referred to as the gas supply system. When metal-containing gas flows through gas supply pipe 310, the metal-containing gas supply system primarily comprises a portion of integrated gas system 20 and gas supply pipe 310, but nozzle 410 may also be considered part of the metal-containing gas supply system. Furthermore, when reducing gas flows through gas supply pipe 320, the reducing gas supply system primarily comprises a portion of integrated gas system 20 and gas supply pipe 320, but nozzle 420 may also be considered part of the reducing gas supply system. Furthermore, when oxygen-containing gas flows through gas supply pipe 330, the oxygen-containing gas supply system primarily comprises a portion of integrated gas system 20 and gas supply pipe 330, but nozzle 430 may also be considered part of the oxygen-containing gas supply system. When a halogen-containing gas flows through the gas supply pipe 340, the halogen-containing gas supply system primarily comprises a portion of the integrated gas system 20 and the gas supply pipe 340. However, the nozzle 440 may also be included in the halogen-containing gas supply system. Alternatively, a portion of the integrated gas system 20 may constitute an inert gas supply system. The inert gas supply system may also be referred to as a rare gas supply system.

[0042] In this embodiment, the gas supply method transports gas through nozzles 410, 420, 430, and 440 disposed within the preparatory chamber 201a, which is a circular, longitudinal space defined by the inner wall of the inner tube 204 and the ends of the plurality of wafers 200. Gas is then ejected into the inner tube 204 from a plurality of gas supply holes 410a, 420a, 430a, and 440a disposed in the nozzles 410, 420, 430, and 440, located opposite the wafers. More specifically, the processing gas, etc., is ejected parallel to the surface of the wafers 200 through the gas supply holes 410a, 420a, 430a, and 440a of the nozzles 410, 420, 430, and 440.

[0043] The exhaust hole (exhaust port) 204a is a through-hole formed in the sidewall of the inner tube 204 at a position opposite the nozzles 410, 420, 430, and 440. For example, it is a slit-shaped through-hole extending in a vertical direction. Gas supplied into the processing chamber 201 from the gas supply holes 410a, 420a, 430a, and 440a of the nozzles 410, 420, 430, and 440 and flowing over the surface of the wafer 200 flows through the exhaust hole 204a into the exhaust path 206. The exhaust path 206 is formed by the gap formed between the inner tube 204 and the outer tube 203. The gas flowing into the exhaust path 206 then flows into the exhaust pipe 231 and is exhausted outside the processing furnace 202.

[0044] The exhaust holes 204a are provided at positions facing the plurality of wafers 200. The gas supplied from the gas supply holes 410a, 420a, 430a, and 440a to the vicinity of the wafers 200 in the processing chamber 201 flows horizontally and then flows through the exhaust holes 204a into the exhaust path 206. The exhaust holes 204a are not limited to being slit-shaped through holes and may be formed of a plurality of holes.

[0045] The manifold 209 is provided with an exhaust pipe 231 for exhausting the atmosphere in the processing chamber 201. The exhaust pipe 231 is connected in order from the upstream side to a pressure sensor 245 (pressure detection unit) that detects the pressure in the processing chamber 201, an APC (Auto Pressure Controller) valve 243, and an exhaust system 700. Figure 2 As shown, the exhaust system 700 is provided with a vacuum pump 246 as a pump, a raw material collection system 702, and a decontamination device 704. The APC valve 243 can be opened and closed while the vacuum pump 246 is in operation to enable and disable vacuum exhaust within the processing chamber 201. Furthermore, the pressure within the processing chamber 201 can be adjusted by adjusting the valve opening while the vacuum pump 246 is in operation. The exhaust system primarily comprises the exhaust hole 204a, the exhaust path 206, the exhaust pipe 231, the APC valve 243, the pressure sensor 245, and the raw material collection system 702 within the exhaust system 700. It is also conceivable that the vacuum pump 246 may also be included in the exhaust system.

[0046] A sealing cover 219, serving as a furnace port cover and capable of airtightly sealing the lower opening of the manifold 209, is provided below the manifold 209. The sealing cover 219 is configured to abut the lower end of the manifold 209 from the vertically downward side. The sealing cover 219 is formed of a metal such as SUS and is disc-shaped. An O-ring 220b, serving as a sealing member, is provided on the upper surface of the sealing cover 219 and abuts the lower end of the manifold 209. A rotating mechanism 267 is provided on the side of the sealing cover 219 opposite the processing chamber 201 to rotate the wafer boat 217 housing the wafers 200. A rotating shaft 255 of the rotating mechanism 267 passes through the sealing cover 219 and is connected to the wafer boat 217. The rotating mechanism 267 is configured to rotate the wafers 200 by rotating the wafer boat 217. The sealing cover 219 is configured to be vertically raised and lowered by a boat elevator 115, serving as an elevating mechanism, disposed vertically outside the outer tube 203. The boat elevator 115 is configured to move the wafer boat 217 into and out of the processing chamber 201 by raising and lowering the seal cap 219. The boat elevator 115 serves as a transport device (transport system) that transports the wafer boat 217 and the wafers 200 accommodated therein into and out of the processing chamber 201.

[0047] The wafer boat 217, which serves as a substrate support, is configured such that a plurality of wafers 200, for example 25 to 200, are arranged in a horizontal position and at intervals in the vertical direction with their centers aligned. The wafer boat 217 is made of, for example, a heat-resistant material such as quartz or SiC. The lower portion of the wafer boat 217 is supported by a heat-insulating tube 218, which is a tubular component made of, for example, a heat-resistant material such as quartz or SiC. This structure makes it difficult for heat from the heater 207 to be transferred to the sealing cover 219 side. However, this embodiment is not limited to the above method. For example, instead of providing the heat-insulating tube 218, a heat-insulating plate made of a heat-resistant material such as quartz or SiC may be supported in multiple stages (not shown) in a horizontal position at the lower portion of the wafer boat 217.

[0048] A temperature sensor (not shown) serving as a temperature detector is provided within inner tube 204. The amount of current supplied to heater 207 is adjusted based on the temperature information detected by the temperature sensor, thereby achieving a desired temperature distribution within processing chamber 201. The temperature sensor, like nozzles 410, 420, 430, and 440, is L-shaped and disposed along the inner wall of inner tube 204.

[0049] like Figure 6As shown, the controller 121, which serves as a control unit (control unit), is a computer configured as follows: a CPU (Central Processing Unit) 121a, a RAM (Random Access Memory) 121b, a storage device 121c, and an I / O port 121d. The RAM 121b, storage device 121c, and I / O port 121d are configured to exchange data with the CPU 121a via an internal bus. The controller 121 is connected to an input / output device 122, such as a touch panel.

[0050] The storage device 121c is composed of, for example, a flash memory, an HDD (Hard Disk Drive), etc. A control program for controlling the actions of the substrate processing device, a process that records the process or conditions of the semiconductor device manufacturing method (substrate processing method) described later, etc. are stored in a readable manner in the storage device 121c. The process is a combination of the processes (steps) in the semiconductor device manufacturing method (substrate processing method) described later by the controller 121 to obtain a predetermined result, and functions as a program. Hereinafter, the process, control program, etc. are collectively referred to as a program. In this specification, when the term "program" is used, there is a case where only a process unit is included, a case where only a control program unit is included, or a case where a combination of a process and a control program is included. RAM121b is configured as a storage area (work area) for temporarily holding programs or data read by CPU121a.

[0051] The I / O port 121 d is connected to the integrated gas system 20 , the pressure sensor 245 , the APC valve 243 , the vacuum pump 246 , the heater 207 , the temperature sensor, the rotation mechanism 267 , the boat elevator 115 , and the like.

[0052] The CPU 121a is configured to read and execute a control program from the storage device 121c, and to read a process from the storage device 121c based on input of an operation command from the input / output device 122. The CPU 121a is configured to control the following operations in accordance with the read process content: flow rate adjustment of various gases by the integrated gas system 20, opening and closing of valves (not shown) included in the integrated gas system 20, opening and closing of the APC valve 243 and pressure adjustment by the APC valve 243 based on the pressure sensor 245, temperature adjustment of the heater 207 based on the temperature sensor, starting and stopping of the vacuum pump 246, rotation of the wafer boat 217 and rotation speed adjustment by the rotation mechanism 267, raising and lowering of the wafer boat 217 by the wafer boat elevator 115, and storage of the wafers 200 into the wafer boat 217.

[0053] The controller 121 can be constructed by installing the above-mentioned program stored in an external storage device (for example, a magnetic disk such as a magnetic tape, a floppy disk, a hard disk, an optical disk such as a CD, a DVD, an optical magnetic disk such as an MO, a USB memory, a semiconductor memory such as a memory card) 123 into a computer. The storage device 121c and the external storage device 123 constitute a computer-readable storage medium. Hereinafter, they are also collectively referred to as storage media. In this specification, the storage medium may include only the storage device 121c alone, only the external storage device 123 alone, or both. It is also possible to provide the program to the computer using a communication unit such as the Internet or a dedicated line instead of using the external storage device 123.

[0054] (2) Structure of the raw material collection system

[0055] exist Figure 2 In FIG. 2 , the raw material collection system 702 includes, for example, an exhaust pipe 231 , a collecting unit 706 , and a heating unit 708 .

[0056] The exhaust pipe 231 is a pipe for exhausting the process gas containing the metal-containing raw material from the process chamber 201 , and includes, for example, a first exhaust line 711 and a second exhaust line 712 .

[0057] The collection section 706 is located in the first exhaust line 711 and is a device that captures the metal-containing raw material from the process gas. A first automatic valve 721, an example of a first valve, and a first manual valve 731 are located upstream of the collection section 706 in the first exhaust line 711. The first manual valve 731 is located downstream of the first automatic valve 721.

[0058] A second manual valve 732 and a second automatic valve 722 are provided as an example of a second valve on the downstream side of the collecting portion 706 in the first exhaust line 711. The second automatic valve 722 is provided on the upstream side of the second manual valve 732.

[0059] Furthermore, a pipe heater (not shown) may be provided in the first exhaust line 711 .

[0060] Heating unit 708 heats collecting unit 706 according to the viscosity of the metal-containing raw material. For example, hot water circulation unit 734 is connected to heating unit 708. By supplying and circulating hot water (heat medium) generated by hot water circulation unit 734 into heating unit 708, heating collecting unit 706 can be achieved by heating unit 708. Heating unit 708 may also be a mantle heater.

[0061] In addition, a cooling unit for cooling the collecting unit 706 may also be provided. The cooling unit is configured to cool the processing gas flowing into the collecting unit 706. In this embodiment, a cold water circulation device 736 is connected to the heating unit 708 in parallel with the hot water circulation device 734. By supplying cold water (heat medium) generated by the cold water circulation device 736 to the heating unit 708 and circulating it, the heating unit 708 can be used as a cooling unit. In other words, the heating unit 708 can also serve as a cooling unit. In this embodiment, this makes it possible to achieve both heating and cooling of the collecting unit 706.

[0062] The cooling temperature is set above the freezing point of the heat medium, so that the equilibrium vapor pressure of the Ru raw material is approximately 90,000 Pa or less. At this point, if the partial pressure of the Ru raw material in the exhaust gas exceeds the equilibrium vapor pressure, condensation will occur. Furthermore, the process gas entering the collection unit 706 is heated to a high temperature due to adiabatic compression by the vacuum pump 246.

[0063] The heat medium flowing through the heating unit 708 may be supplied from the lower side to the upper side of the collecting unit 706. The same is true when the heating unit 708 is used as a cooling unit. In this way, the processing gas can be efficiently heated or cooled.

[0064] Valves 741 and 742 are provided on the upstream and downstream sides of the hot water circulation system 734, respectively, in the piping connecting the hot water circulation system 734 and the heating unit 708. Furthermore, valves 751 and 752 are provided on the upstream and downstream sides of the cold water circulation system 736, respectively, in the piping connecting the cold water circulation system 736 and the heating unit 708. Valves 741 and 751 are provided in parallel with each other. Valves 742 and 752 are also provided in parallel with each other.

[0065] The collecting section 706 is configured so that the metal-containing raw material does not undergo phase change due to heating by the heating section 708. This can suppress resublimation of the raw material and improve recovery efficiency.

[0066] The heating of the collecting portion 706 by the heating portion 708 is adjusted so that the metal-containing raw material has a viscosity that allows it to flow in the direction of gravity in the collecting portion 706. This can improve the recovery efficiency of the metal-containing raw material.

[0067] Furthermore, the temperature of the heating unit 708 is set so that the viscosity of the metal-containing raw material becomes equal to or lower than a predetermined viscosity and the vapor pressure becomes equal to or lower than a predetermined pressure.

[0068] The viscosity of the Ru raw material used in the metal-containing raw material (metal-containing gas) varies significantly around room temperature. For example, the viscosity varies from approximately 380 cP (at 25°C) to approximately 90 cP (at 40°C). The heating performed by the heating unit 708 is set to a temperature below approximately 100 cP, a viscosity that allows the material to drip into the reservoir 710 due to the flow of the process gas and gravity. Consider a droplet hanging on a vertical plate.

[0069] The collecting portion 706 may be heated not only during collection but also periodically when the particles adhere to the surface and the heat exchange efficiency is reduced.

[0070] Regarding temperature control, there are the following methods: a method of controlling the temperature of the heat medium by assuming that the temperature of the heat medium is approximately equal to the temperature of the collector condensing surface; a method of controlling the flow rate or temperature of the heat medium so that the temperature of a sensor installed near the condensing surface reaches a set temperature.

[0071] The raw material collection system 702 may further include a vacuum pump 246. The vacuum pump 246 is disposed in the exhaust pipe 231 between the processing chamber 201 and the first exhaust line 711, for example, between the branch between the first exhaust line 711 and the second exhaust line 712. It is an example of a pump that performs vacuum exhaust of the process gas. In this case, the collection unit 706 is disposed on the secondary side (exhaust side) of the vacuum pump 246. Alternatively, an inert gas may be supplied to the vacuum pump 246 via the piping 250 and valve 252.

[0072] The second exhaust line 712 is installed in the exhaust pipe 231 to bypass the first exhaust line 711. A valve 714 is installed in the second exhaust line 712. A detoxification device 740 for detoxifying the process gas flowing through the exhaust pipe 231 can be installed downstream of the collection section 706 in the exhaust pipe 231, specifically downstream of the confluence of the second exhaust line 712 and the first exhaust line in the exhaust pipe 321. The second exhaust line 712 bypasses the collection section 706 and connects the vacuum pump 246 to the detoxification device 740.

[0073] The entire pipe from the vacuum pump 246 to the abatement device 740 , specifically, the entire pipe from the vacuum pump 246 to the abatement device 740 via the second exhaust line 712 , may be heated by, for example, the pipe heater 713 .

[0074] The treatment gas exhausted to the atmosphere can be rendered harmless by the detoxification device 740. In addition, the second exhaust line 712 is used to bypass the collection unit 706 when the treatment gas is not extended, thereby suppressing the re-sublimation of the metal-containing raw material after repairing the collection unit 706.

[0075] The raw material collection system 702 may include a storage unit 710 for recovering the metal-containing raw material. The storage unit 710 is connected to the downward direction of the gravity of the collection unit 706. The metal-containing raw material in the collection unit 706 is heated by the heating unit 708 and then recovered in the storage unit 710. This allows for efficient recovery of the metal-containing raw material.

[0076] like Figure 3 As shown, the collection section 706 and the storage section 710 can be linearly connected by connecting the ports 754a and 754b facing each other on the T-branch pipe 754. In this case, the processed gas is discharged from the port 754c that does not face the ports 754a and 754b of the T-branch pipe. This allows the metal-containing raw material captured by the collection section 706 to drip efficiently into the storage section 710, while also enabling efficient exhaust.

[0077] In addition, if Figure 8 As shown, the T-branch pipe 754 may not be used, and the downstream side of the collecting section 706 in the first exhaust line 711 may be connected to the collecting section 706 .

[0078] A connection 707 may be provided to connect the collecting section 706 and the storage section 710. This connection 707 is, for example, a flange provided at the connection between the outlet 58 of the collecting section 706 and the port 754a of the T-branch pipe 754. The connection 707 may be configured to prevent the metal-containing raw material from adhering to the sidewall of the storage section 710.

[0079] As an example, the connecting portion 707 may be provided with a guide portion 760 configured to guide the metal-containing raw material to the bottom of the storage portion 710 ( Figure 5 The guide portion 760 includes, for example, a circular portion 762 and a funnel portion 764, which are attached to the inner side of the connecting portion 707. The funnel portion 764 is secured to the inner circumference of the circular portion 762 and is vertically open, tapering from the upper end toward the lower end. This improves the recovery efficiency of the metal-containing raw material.

[0080] The processing gas inlet 56 is provided at the upper end of the collecting section 706, and the processing gas outlet 58 is provided at the lower end of the collecting section 706. Furthermore, the processing gas is configured to flow downward from the inlet 56 to the outlet 58 within the collecting section 706. As a result, the metal-containing raw material drips from the outlet 58 into the reservoir 710.

[0081] As described above, the collecting portion 706 can be cooled by a refrigerant. In this case, a gas contact surface for condensing the liquid metal raw material can be formed on a vertical surface in the collecting portion 706. Figure 4A In the embodiment, the collecting portion 706 includes, for example, a heat transfer tube housing shell 50. Figure 4BAs shown, the heat transfer tube housing 50 surrounds and houses a plurality of heat transfer tubes 51, which are regularly arranged in parallel with small intervals. The heat transfer tubes 51 are formed, for example, into a petal-shaped cross-section. In this example, all the heat transfer tubes 51 are straight, but they can also be curved. Except for the heat transfer tubes arranged at the outermost periphery, these heat transfer tubes 51 are arranged so that any grooves face each other. This arrangement allows the heat transfer tubes 51 having the cross-sectional structure described in the various embodiments to be bundled at the highest density.

[0082] The heat transfer tube housing 30 in the figure is provided with connectors 36 and 37 for connecting the connection ends 12 of a plurality of heat transfer tubes together and communicating with the interior 63 of the heat transfer tubes. At the same time, a passage 64 is provided with a small gap formed between the heat transfer tubes 51 and the heat transfer tubes 51 and between the heat transfer tubes 51 and the heat transfer tube housing 50. In the example of the figure, for example, the processing gas is introduced into the connector (in) 52 through the inlet 56, and the processing gas reaches the connector (out) 53 through the interior 63 of the heat transfer tubes and is discharged from the outlet 58. The condensed metal-containing raw material is recovered to the storage part 710, and the remaining gas is sent to the detoxification device 740 ( Figure 1 On the other hand, for example, heat medium is introduced from the heat medium inlet 61 and discharged from the heat medium outlet 60 through the passage 64 .

[0083] (3) Substrate processing step (substrate processing method)

[0084] As one of the steps in the manufacturing process of a semiconductor device, Figure 7 An example process of forming a metal-containing film containing a metal element on a wafer 200 on which a metal-containing film containing a metal element has been formed as a base film will be described. The process of forming the metal-containing film on the wafer 200 on which the metal-containing film has been formed is performed using the processing furnace 202 of the aforementioned substrate processing apparatus 10. In the following description, the operations of the various components constituting the substrate processing apparatus 10 are controlled by the controller 121.

[0085] The substrate processing step (semiconductor device manufacturing step) of this embodiment includes the following steps:

[0086] (a) supplying a metal-containing gas containing a metal element to the wafer 200 on which the metal-containing film is formed;

[0087] (b) supplying a reducing gas to the wafer 200;

[0088] (c) supplying an oxygen-containing gas containing oxygen atoms and the reducing gas to the wafer 200;

[0089] (d) repeating the cycle consisting of (a) and (b) a first number of times; and

[0090] (e) After (d), repeat the loop consisting of (a) and (c) a second time.

[0091] In this specification, when the term "wafer" is used, it may refer to "the wafer itself" or "a laminate of a wafer and a predetermined layer or film formed on its surface." In this specification, when the term "surface of a wafer" is used, it may refer to "the surface of the wafer itself" or "the surface of a predetermined layer or film formed on the wafer." In this specification, when the term "substrate" is used, it has the same meaning as when the term "wafer" is used.

[0092] (Wafer loading)

[0093] When multiple wafers 200 are loaded (wafer loading) into the wafer boat 217, as shown in FIG. Figure 1 As shown, the wafer boat 217 supporting the plurality of wafers 200 is lifted by the wafer boat elevator 115 and carried into the processing chamber 201 (wafer boat loading) and stored in the processing container. In this state, the seal cap 219 is in a state of sealing the lower end opening of the outer tube 203 via the O-ring 220.

[0094] (Pressure adjustment and temperature adjustment)

[0095] The vacuum pump 246 evacuates the processing chamber 201, i.e., the space where the wafers 200 are located, to a desired pressure (vacuum level). At this point, the pressure within the processing chamber 201 is measured by the pressure sensor 245. Feedback control (pressure adjustment) of the APC valve 243 is performed based on this measured pressure information. The vacuum pump 246 remains in operation until at least the processing of the wafers 200 is completed.

[0096] Furthermore, the processing chamber 201 is heated by heater 207 to a desired temperature. At this time, the amount of current supplied to heater 207 is feedback-controlled (temperature adjusted) based on the temperature information detected by the temperature sensor to achieve a desired temperature distribution within the processing chamber 201. The heating of the processing chamber 201 by heater 207 continues at least until the processing of the wafers 200 is completed.

[0097] Here, as the metal-containing film serving as the base film, a film containing at least one of tungsten (W), molybdenum (Mo), copper (Cu), and cobalt (Co) as a metal element and a transition metal (transition element) can be used. The metal-containing film can be used as metal wiring. The metal-containing film can be the bottom metal wiring M1 of the wiring layer or the metal wiring My (where y is a natural number) in an intermediate layer.

[0098] For example, a metal-containing film is formed on the wafer 200, an insulating film is formed on the metal-containing film, and when the metal-containing film containing metal elements is embedded in the recess on the wafer 200 where the insulating film forms recesses such as grooves or holes, a metal oxide film as a natural oxide film is sometimes formed on the surface of the metal-containing film in the recess. In particular, transition metals such as W, Mo, Cu, and Co are easily oxidized and sometimes form a metal oxide film on the surface. If a metal oxide film is formed but is not removed and remains, the contact resistance between the metal-containing film and the metal-containing film embedded in the recess may increase. In the case of forming a ruthenium (Ru) film as an example of a metal-containing film, in order to give play to the low resistance of the Ru film, the contact resistance must be reduced.

[0099] Therefore, in the substrate processing step (semiconductor device manufacturing step) of this embodiment, before forming the metal-containing film within the recessed portion, a pretreatment step is performed within the same processing chamber 201. A halogen-containing gas containing a halogen element is supplied to the wafer 200 to remove at least a portion of the metal oxide film. In other words, the pretreatment step and the film formation step are performed continuously within the same processing chamber (in situ). Specifically, after the metal oxide film is removed by the pretreatment step, the film formation step is performed within the same processing chamber 201 to form the metal-containing film.

[0100] A. Pretreatment process

[0101] (Supplying halogen-containing gas, step S1)

[0102] Illustration of symbols for each step is omitted. Valve 344 is opened to allow the halogen-containing gas to flow through the gas supply pipe 340. The halogen-containing gas is flow-regulated by MFC 342 and supplied from the gas supply hole 440a of the nozzle 440 into the processing chamber 201 and exhausted through the exhaust pipe 231. At this time, the halogen-containing gas is supplied to the wafer 200. At the same time, valve 544 is opened to allow the inert gas to flow through the gas supply pipe 540. The inert gas flowing through the gas supply pipe 540 is flow-regulated by MFC 542 and supplied into the processing chamber 201 along with the halogen-containing gas and exhausted through the exhaust pipe 231. At this time, to prevent the halogen-containing gas from entering the nozzles 410, 420, and 430, valves 514, 524, and 534 are opened to allow the inert gas to flow through the gas supply pipes 510, 520, and 530. An inert gas is supplied into the processing chamber 201 through the gas supply pipes 310 , 320 , 330 and the nozzles 410 , 420 , 430 , and is exhausted from the exhaust pipe 231 .

[0103] At this time, adjust the APC valve 243 so that the pressure in the processing chamber 201 is, for example, within the range of 1 to 3990 Pa. The supply flow rate of the halogen-containing gas controlled by MFC342 is, for example, within the range of 0.05 to 20 slm. The supply flow rates of the inert gas controlled by MFC512, C522, 532, and 542 are, for example, within the range of 0.1 to 50 slm. In addition, the expression of a numerical range such as "1 to 3990 Pa" in this disclosure means that the lower limit and the upper limit are included in the range. Therefore, for example, "1 to 3990 Pa" means "above 1 Pa and below 3990 Pa". The same applies to other numerical ranges.

[0104] At this time, the gases flowing within processing chamber 201 are only the halogen-containing gas and the inert gas. The halogen-containing gas undergoes a substitution reaction with at least a portion of the metal oxide film formed on the metal-containing film. Specifically, oxygen in the metal oxide film reacts with the halogen element, desorbing from the metal oxide film and being discharged from processing chamber 201 as a reaction byproduct. In other words, at least a portion of the metal oxide film is removed (etched).

[0105] As the halogen-containing gas, for example, a gas capable of selectively etching only the metal oxide film formed in the recessed portion on the wafer 200 can be used. As the halogen-containing gas, a gas containing, for example, one or more chlorine (Cl) atoms and one or more oxygen (O) atoms as halogen elements can be used. That is, as the halogen-containing gas, a gas having a molecular structure of MO can be used. x Cl y Here, M includes, for example, at least one of phosphorus (P), sulfur (S), and carbon (C). Examples of oxyhalides include phosphorus oxychloride (POCl3), thionyl chloride (SOCl2), and phosgene (COCl2). Halogen-containing gases may include at least one of these gases.

[0106] Thus, when an oxyhalide is used as the halogen-containing gas, the O in the metal oxide film reacts with Cl and O, being removed from the metal oxide film, and selectively etching only the metal oxide film. For example, it is possible to selectively etch only the metal oxide film without etching an insulating film formed of a silicon oxide (SiO2) film. In other words, a halogen-containing gas can also be referred to as an etching gas that etches metal oxide films.

[0107] (Removal of residual gas (exhaust), step S2)

[0108] After a predetermined time, for example, 1 to 600 seconds, has passed since the start of the supply of the halogen-containing gas, the supply of the halogen-containing gas from the gas supply pipe 340 is stopped. That is, the time for supplying the halogen-containing gas to the wafer 200 is, for example, 1 to 600 seconds. At this time, the APC valve 243 of the exhaust pipe 231 remains open, and the processing chamber 201 is vacuum-exhausted by the vacuum pump 246 to remove the halogen-containing gas remaining in the processing chamber 201 that has not reacted or has contributed to the etching of the metal oxide film from the processing chamber 201 (the space where the wafer 200 is located is exhausted). That is, the processing chamber 201 is purged. At this time, the supply of inert gas to the processing chamber 201 is maintained. The inert gas acts as a purge gas, which can improve the effect of removing the halogen-containing gas remaining in the processing chamber 201 that has not reacted or has contributed to the etching from the processing chamber 201.

[0109] In addition, the above-mentioned pretreatment step may also be referred to as a metal oxide film removal step, a pre-etching step, or a pre-cleaning step.

[0110] B. Metal-containing film forming step (film forming step)

[0111] [First Metal-Containing Film Formation Step]

[0112] (Supplying Metal-Containing Gas, Step S11)

[0113] A metal-containing gas, serving as a raw material gas, flows from the integrated gas system 20 into the gas supply pipe 310. The metal-containing gas has its flow rate adjusted in the integrated gas system 20 and is supplied into the processing chamber 201 through the gas supply hole 410a of the nozzle 410 and exhausted through the exhaust pipe 231. Simultaneously, an inert gas flows from the integrated gas system 20 into the gas supply pipe 310. The inert gas has its flow rate adjusted in the integrated gas system 20 and is supplied into the processing chamber 201 along with the metal-containing gas and exhausted through the exhaust pipe 231. To prevent the metal-containing gas from entering the nozzles 420, 430, and 440, the inert gas flows out of the integrated gas system 20. The inert gas is supplied into the processing chamber 201 through the gas supply pipes 320, 330, and 340 and the nozzles 420, 430, and 440 and exhausted through the exhaust pipe 231.

[0114] At this time, the pressure in the processing chamber 201 is maintained within a range of, for example, 1 to 3990 Pa by the integrated gas system 20. The metal-containing gas is supplied at a flow rate of, for example, 0.05 to 1 slm. The inert gas is supplied at a flow rate of, for example, 0.1 to 50 slm.

[0115] At this time, the gases flowing within processing chamber 201 are only metal-containing gas and inert gas. Specifically, the metal-containing gas is supplied to wafer 200, from which the metal oxide film has been removed, to form a metal-containing layer on wafer 200 (including the insulating film on the surface and within the recessed portion). The metal-containing layer can be a metal layer containing other elements or an adsorbed layer of the metal-containing gas.

[0116] As the metal-containing gas, for example, a gas containing a transition metal (transition element) as a metal element can be used, preferably a platinum group element, and a gas containing a Group VIII element can be used. As the metal-containing gas, for example, a Ru-containing gas containing ruthenium (Ru) can be used. In this way, by using a gas containing a transition metal, a platinum group element, and a Group VIII element, a low-resistance metal-containing film can be formed. In addition, as the metal-containing gas, a gas containing a metal element and a carbonyl group can be used. This can increase the film formation rate.

[0117] As the metal-containing gas, for example, a gas obtained by vaporizing the following organometallic materials can be used: bisethylcyclopentadienylruthenium (Ru(C2H5C5H4)2), butylpentenylruthenium (Ru(C5H5)(C4H9C5H4), tris-2,4-octanedionatoruthenium (Ru[CH3COCHCO(CH2)3CH3]3), 2,4-dimethylcyclopentadienylethylcyclopentadienylruthenium (Ru(C2H5C5H4)((CH3)C5H5)), Ru(C7H8)(C7H 11 O2), dicarbonylbis(5-methyl-2,4-hexanedione)ruthenium(II) (C 16 H 22 O6Ru), triruthenium dodecacarbonyl (Ru3(CO) 12 ), η4-2,3-dimethylbutadienyl ruthenium tricarbonyl ((DMBD)Ru(CO)3), η4-butadienyl ruthenium tricarbonyl ((BD)Ru(CO3)), η4-1,3-cyclohexadienyl ruthenium tricarbonyl ((CHD)Ru(CO)3), bis(cyclopentadienyl ruthenium dicarbonyl (C 14 H 10 O4Ru2)), tricarbonyldichlororuthenium (II) [(Ru(CO)3Cl2)2], etc. As the metal-containing gas, one or more of these gases can be used.

[0118] Here, when Ru-containing gas is used as the metal-containing gas, for example, a Ru-containing layer is formed in the recess on the wafer 200. The Ru-containing layer may be a Ru layer containing other elements, an adsorption layer of Ru-containing gas, or both.

[0119] (Removing Residual Gas, Step S12)

[0120] After a predetermined time, for example, 1 to 120 seconds, has passed since the start of the supply of the metal-containing gas, the supply of the metal-containing gas from the gas supply pipe 310 is stopped. That is, the time for supplying the metal-containing gas to the wafer 200 is, for example, 1 to 120 seconds. At this time, the processing chamber 201 is evacuated using the vacuum pump 246 to remove the metal-containing gas remaining in the processing chamber 201 that has not reacted or has contributed to the formation of the metal-containing layer. In other words, the processing chamber 201 is purged. At this time, the supply of inert gas to the processing chamber 201 is maintained. The inert gas acts as a purge gas, which can improve the effect of removing the metal-containing gas remaining in the processing chamber 201 that has not reacted or has contributed to the formation of the metal-containing layer.

[0121] (Supplying Reducing Gas, Step S13)

[0122] After the residual gas in the processing chamber 201 is removed, reducing gas flows from the integrated gas system 20 into the gas supply pipe 320. The reducing gas is flow-controlled in the integrated gas system 20 and supplied into the processing chamber 201 through the gas supply hole 420a of the nozzle 420 and exhausted through the exhaust pipe 231. At this time, reducing gas is supplied to the wafers 200. At the same time, an inert gas flows from the integrated gas system 20 into the gas supply pipe 320. The flow rate of the inert gas is controlled in the integrated gas system 20. The inert gas is supplied into the processing chamber 201 along with the reducing gas and exhausted through the exhaust pipe 231. At this time, the inert gas is allowed to flow to prevent the reducing gas from entering the nozzles 410, 430, and 440. The inert gas is supplied into the processing chamber 201 through the gas supply pipes 310, 330, 340 and the nozzles 410, 430, and 440 and exhausted through the exhaust pipe 231.

[0123] At this time, the pressure in the processing chamber 201 is maintained within a range of, for example, 5 to 15,000 Pa by the integrated gas system 20. The reducing gas is supplied at a flow rate of, for example, 1 to 100 slm, preferably 15 to 50 slm. The inert gas is supplied at a flow rate of, for example, 0.1 to 50 slm.

[0124] Here, the pressure in the processing chamber 201 in this step, that is, the pressure (total pressure) in the space where the wafer 200 is located, is set higher than the pressure (total pressure) in the space where the wafer 200 is located in step S23 described later. In other words, the pressure in the processing chamber 201 in this step is set higher than the pressure in the processing chamber 201 in step S23 described later.

[0125] By increasing the pressure in the processing chamber 201 when supplying the reducing gas, ligands in the film can be easily removed. If a high pressure purge is performed during the removal of residual gas in step S12 to remove the ligands, it will take time for the pressure in the processing chamber 201 to return to its original pressure. By increasing the pressure in the processing chamber 201 during the supply of the reducing gas in this step, the ligands can be removed (purged) in a shorter time than when the pressure in the processing chamber 201 is increased.

[0126] Furthermore, if the pressure in processing chamber 201 is kept high during the supply of reducing gas in all steps of the substrate processing process, a pressure adjustment time from low pressure to high pressure is required between the supply of the metal-containing gas and the supply of the reducing gas. In the present disclosure, the pressure in processing chamber 201 is increased to high pressure during the supply of reducing gas in the first half of the process (forming the first metal-containing film), and is reduced to low pressure during the supply of reducing gas in the second half (forming the second metal-containing film). This shortens the pressure adjustment time between the supply of the metal-containing gas and the supply of the reducing gas, thereby improving productivity.

[0127] Furthermore, the partial pressure of the reducing gas in this step may be higher than the partial pressure of the reducing gas in step S23 described later. Furthermore, at least one of the pressure in the processing chamber 201 and the partial pressure of the reducing gas in this step may be varied every predetermined number of cycles (a first number of cycles). In other words, at least one of the pressure in the processing chamber 201 during the supply of the reducing gas in this step and the partial pressure of the reducing gas may be varied every predetermined number of cycles (a first number of cycles) of repeating the first metal-containing film formation step. Specifically, at least one of the pressure in the processing chamber 201 and the partial pressure of the reducing gas in this step may be reduced every predetermined number of cycles (a first number of cycles).

[0128] At this time, the gases flowing in the processing chamber 201 are only the reducing gas and the inert gas.

[0129] As the reducing gas, for example, hydrogen (H)-containing gas, hydrogen (H 2 ) gas, deuterium (D 2 ) gas, gas containing activated hydrogen, etc. As the reducing gas, one or more gases among these can be used.

[0130] Here, when H2 gas is used as the reducing gas, the H2 gas undergoes a substitution reaction with at least a portion of the metal-containing layer formed on the wafer 200 in step S11. For example, when a gas containing a metal element and a carbonyl group is used as the metal-containing gas, O and the like in the metal-containing layer react with H2, desorb from the metal-containing layer, and are exhausted from the processing chamber 201 as reaction byproducts such as water vapor (H2O). Thus, a metal-containing layer containing metal elements and reduced in O is formed on the wafer 200.

[0131] (Removing Residual Gas, Step S14)

[0132] After the metal-containing layer is formed, the supply of the reducing gas is stopped. Then, through the same process as step S12 described above, any remaining reducing gas or reaction byproducts that have not reacted or have contributed to the formation of the metal-containing layer are removed from the processing chamber 201. In other words, the processing chamber 201 is purged.

[0133] (Specified number of implementations)

[0134] By sequentially performing the above-described cycle of steps S11 to S14 at least once (a first number (predetermined number) (n times)), a first metal-containing film having a predetermined thickness is formed on the wafer. The above-described cycle is preferably repeated multiple times. This can reduce the amount of surface oxide layer on the metal-containing film, and can form a first metal-containing film that suppresses the growth of oxide layer at the interface.

[0135] (Post-purge and restoration of atmospheric pressure)

[0136] Inert gas is supplied into the processing chamber 201 from the gas supply pipes 510 to 540 and exhausted from the exhaust pipe 231. The inert gas acts as a purge gas, thereby purging the processing chamber 201 with the inert gas and removing any gas or reaction byproducts remaining in the processing chamber 201 (post-purge). Afterwards, the atmosphere in the processing chamber 201 is replaced with the inert gas (inert gas replacement), and the pressure in the processing chamber 201 is restored to normal pressure (atmospheric pressure recovery).

[0137] (Wafer removal)

[0138] The sealing cap 219 is then lowered by the boat elevator 115, opening the lower end of the outer tube 203. The processed wafers 200, supported by the boat 217, are then unloaded from the lower end of the outer tube 203 (boat unloading). The processed wafers 200 are then removed from the boat 217 (wafer unloading).

[0139] That is, in the substrate processing step of the present disclosure, the first metal-containing film forming step forms, on the wafer 200 having the metal-containing film formed on its surface, a first metal-containing film that suppresses growth of an oxide layer at the interface on the metal-containing film.

[0140] (4) Raw material collection method

[0141] exist Figure 1 、 Figure 2 The raw material collection method of this embodiment has the following steps:

[0142] exhausting the process gas containing the metal-containing raw material from the process chamber 201 through the exhaust pipe 231;

[0143] The collecting portion 706 provided in the first exhaust line 711 constituting the exhaust pipe 231 captures the metal-containing raw materials from the process gas; and

[0144] The collecting portion 706 is heated by the heating portion 708 according to the viscosity of the metal-containing raw material, so that the metal-containing raw material in the collecting portion 706 drips outward.

[0145] exist Figure 2 In the process, the processing gas exhausted from the processing chamber 201 is sucked by the vacuum pump 246 and flows into the exhaust system 700. Here, the valve 714 is closed, and the first automatic valve 721, the first manual valve 731, the second manual valve 732 and the second automatic valve 722 are opened, thereby introducing the processing gas into the collection part 706 to capture the metal-containing raw material. These valves are Figure 7 The supply of the metal-containing gas (process gas containing the metal-containing raw material) is turned on. At this time, the collection portion 706 is heated by the heating portion 708 according to the viscosity of the metal-containing raw material, using, for example, a hot water circulation device 734, so that the metal-containing raw material in the collection portion 706 drips outward, for example, into the storage portion 710.

[0146] exist Figure 3 The internal arrangement of the connecting portion 707 is shown Figure 5 In the case of the guide portion 760 shown, the metal-containing raw material collected by the collecting portion 706 can be directed to the bottom of the reservoir 710. This can prevent the metal-containing raw material from adhering to the inner peripheral wall of the reservoir 710, and can efficiently recover the liquid dripping from the collecting portion 706.

[0147] In this embodiment, the raw material is not decomposed but recovered in its raw material state, thereby reducing the cost and energy consumption during re-refining.

[0148] In the collecting section 706, in order to minimize the resublimation of the raw material when recovering the metal-containing raw material, a cold water circulation device 736 may be used to cool the collecting section 706. By cooling the collecting section 706, the metal-containing raw material can be condensed and liquefied for collection.

[0149] The processed gas that has passed through the collecting portion 706 is detoxified by the detoxification device 740 through the T-branch pipe 709 and then discharged into the atmosphere.

[0150] When the raw materials are not being recovered, to prevent the captured metal-containing raw materials from re-subliming, the process gas is not fed into the collection unit 706. Specifically, the first and second automatic valves 721 and 722 are closed, and valve 714 is opened, switching the exhaust path of the process gas to the second exhaust line 712. This allows the process gas to flow to the detoxification device 740 instead of the collection unit 706.

[0151] When cleaning the processing furnace 202, the metal-containing raw material (precious metal) adhering to the processing chamber 201 is recovered. In addition, the cleaning gas is prevented from flowing into the collecting portion 706. This is to prevent the recovered metal-containing raw material from decomposing.

[0152] During maintenance, the collecting portion 706 may be heated slightly for a short period of time so that the metal-containing raw materials captured by the collecting portion 706 can be collected in the storage portion 710 .

[0153] In addition, the first automatic valve 721 of the raw material capture system 702 is not limited to switching according to the type of gas within the supply cycle of the processing gas, and the processing gas can always pass through the collection part 706 during film formation, or at least the exhaust gas during gas cleaning can bypass the collection part 706.

[0154] (Replacement of the collection and storage parts)

[0155] like Figure 8 As in the illustrated example, the collection portion 706 may be configured to be disconnected from the first exhaust line 711 by closing the first valve and the second valve.

[0156] A first detachable portion 771 may be provided between the first automatic valve 721 and the first manual valve 731 , and a second detachable portion 772 may be provided between the second automatic valve 722 and the second manual valve 732 .

[0157] The replacement process of the collecting section 706 and the storage section 710 is as follows, for example.

[0158] 1. Fill the first exhaust line with inert gas (purge). While the collection section 706 is connected to the decontamination device 740, inject inert gas directly into the ballast port (piping 250) of the vacuum pump 246 or the first exhaust line 711. Close the first and second automatic valves 721 and 722, and while the collection section 706 is sealed with inert gas at approximately atmospheric pressure, heat the collection section 706 for a predetermined time. If heating could potentially cause the pressure to rise above atmospheric pressure, sealing is not necessary.

[0159] 2. Switch the collecting section 706 to cooling mode. Alternatively, this operation may be omitted.

[0160] 3. Stop cooling the collection section 706 and remove the cooling water pipe from the collection section 706. Figure 1 The piping connecting the heating unit 708 and the cold water circulation device 736 is shown in the figure.

[0161] 4. A simple glove box 774 is installed around the collection section 706 and storage section 710.

[0162] 5. After the first exhaust line 711 is purged with the inert gas again, close the first automatic valves 721AV261 and 262. This operation can also be omitted.

[0163] 6. Close the first manual valve 731 and the second manual valve 732.

[0164] 7. Release the flange connection between the collecting part 706 and the first exhaust line 711, and the flange connection between the T-branch pipe 754 and the first exhaust line 711, as shown in FIG. Figure 3 As shown, the collecting portion 706 and the storage portion 710 are removed from the first exhaust line 711 .

[0165] 8. The flanges of the unloaded collecting portion 706 and the storage portion 710 are blocked and protected by a blank flange or the like (not shown). In addition, the unloaded collecting portion 706 and the storage portion 710 are cleaned to recover the metal-containing raw material.

[0166] 9. Connect the new collecting section 706 and storage section 710 to the first exhaust line 711 .

[0167] 10. Connect the cooling water pipe to the collection part 706.

[0168] By removing the collecting section 706 and the storage section 710 from the first exhaust line 711, the raw material recovered by the storage section 710 and the raw material remaining in the collecting section 706 without dripping into the storage section 710 can be easily recovered. In addition, since no valve is provided between the storage sections 710, the raw material liquid condensed in the collecting section 706 can be prevented from accumulating on the valve.

[0169] (Variation)

[0170] exist Figure 2 In the example, a first manual valve 731 and a second manual valve 732 are provided in the first exhaust line 711, but Figure 9 In this modification, a third automatic valve 723 and a third manual valve 733 are provided between the collecting portion 706 and the storage portion 710 .

[0171] In this example, the start and stop of the recovery of the metal-containing raw material repaired in the collection section 706 to the storage section 710 can be switched by opening and closing the third automatic valve 723 and the third manual valve 733 .

[0172] (Substrate processing equipment)

[0173] The substrate processing apparatus 10 includes:

[0174] a processing chamber 201 for processing a substrate disposed therein;

[0175] a metal-containing gas supply system for supplying a process gas containing a metal-containing raw material into the process chamber 201; and

[0176] The raw material capture system 702 captures the metal-containing raw material from the process gas exhausted from the process chamber 201 by the vacuum pump 246.

[0177] The raw material capture system 702 has:

[0178] an exhaust pipe 231 for guiding the exhausted process gas;

[0179] a collecting portion 706 , which is provided in the first exhaust line 711 constituting the exhaust pipe 231 and recovers the metal-containing raw materials from the processed gas; and

[0180] The heating unit 708 heats the collecting unit 706 according to the viscosity of the metal-containing raw material.

[0181] (Method for Manufacturing Semiconductor Device)

[0182] The method for manufacturing a semiconductor device includes the following steps:

[0183] A gaseous metal-containing raw material containing a metal element is supplied into the processing chamber 201 to form a film containing the metal element on the substrate in the processing chamber 201;

[0184] exhausting the process gas containing the metal-containing raw material from the process chamber 201 through the exhaust pipe 231;

[0185] The collecting portion 706 provided in the first exhaust line 711 constituting the exhaust pipe 231 captures the metal-containing raw materials from the process gas; and

[0186] The collecting portion 706 is heated by the heating portion 708 according to the viscosity of the metal-containing raw material, so that the metal-containing raw material in the collecting portion 706 drips outward.

[0187] (5) Effects of this embodiment

[0188] According to the substrate processing apparatus 10 of the present embodiment, one or more of the following effects can be obtained.

[0189] (a) By forming the first metal-containing film, a metal-containing film can be formed in which growth of an oxide layer at the interface on the metal-containing film is suppressed.

[0190] (b) Furthermore, by optimizing the number of cycles in the step of forming the first metal-containing film (the thickness of the first metal-containing film), it is possible to form an improved metal-containing film that achieves both suppression of the oxide layer and reduction of impurities in the film.

[0191] (d) Furthermore, by performing a pretreatment step before the film formation step, the contact resistance between the metal-containing film and the metal-containing film embedded in the recess can be reduced.

[0192] Furthermore, according to the raw material collection system 702 of this embodiment, one or more of the following effects can be obtained.

[0193] (e) The collected raw materials can be efficiently recovered without gasification or deterioration.

[0194] (f) The exhaust speed is not reduced by the collecting portion 706. In addition, the collecting portion 706 can be constructed to be lightweight.

[0195] (g) The flow of the exhaust gas may be utilized to cause the collected liquid to drip into the storage portion 710 below.

[0196] (h) Since the exhaust gas flows parallel to the heat exchange plates (gas contact surface), conductivity can be reduced, allowing for a compact and lightweight collector 706, making installation and replacement easier. Since the heat exchange plates are vertical, droplets flow most easily.

[0197] (6) Other Implementation Methods

[0198] The embodiments of the present disclosure have been described in detail above. However, the present disclosure is not limited to the above embodiments, and various modifications can be made without departing from the spirit thereof. In addition, in the following modified examples, only the differences from the above embodiments are described in detail.

[0199] Furthermore, in the above embodiment, an example in which a predetermined film is formed on the wafer 200 has been described, but the type of film in the present disclosure is not particularly limited.

[0200] In addition, in the above embodiment, an example of using a batch-type vertical device, i.e., a substrate processing device, to form a film is described, but the present disclosure is not limited to this and can also be appropriately applied to the case of using a single-chip substrate processing device that processes one or several substrates at a time to form a film.

[0201] Preferably, a process (a program that records the process or process conditions, etc.) used for substrate processing is prepared separately according to the processing content (film type, composition ratio, film quality, film thickness, processing process, processing conditions, etc. of the film to be formed) and stored in the storage device 121c via an electrical communication line or an external storage device 123. Furthermore, preferably, when starting substrate processing, the CPU 121a appropriately selects a suitable process from the multiple processes stored in the storage device 121c according to the processing content. In this way, films of various film types, composition ratios, film qualities, and film thicknesses can be formed with good reproducibility using one substrate processing device. In addition, the burden on the operator (the burden of inputting the process or process conditions, etc.) can be reduced, operational errors can be avoided, and substrate processing can be started quickly.

[0202] The above-mentioned process recipes are not limited to newly created ones; for example, they can also be prepared by modifying an existing recipe already installed in a substrate processing apparatus. When modifying a recipe, the modified recipe can be installed in the substrate processing apparatus via an electrical communication line or a storage medium containing the recipe. Alternatively, the input / output device 122 of the existing substrate processing apparatus can be used to directly modify the existing recipe installed in the apparatus.

[0203] In this specification, the temperature refers to the temperature of the wafer 200 or the temperature in the processing chamber 201, and the pressure refers to the pressure in the processing chamber 201. In addition, the processing time refers to the time during which the processing is continued.

[0204] In the above embodiment, an example of forming a film using a substrate processing apparatus having a cold-wall processing furnace is described. However, the present disclosure is not limited to the above embodiment and can also be appropriately applied to forming a film using a substrate processing apparatus having a hot-wall processing furnace.

Claims

1. A raw material capture system, characterized in that: have: an exhaust pipe that exhausts a process gas containing a metal-containing raw material from the process chamber and has a first exhaust line; a collecting portion, which is provided in the first exhaust line and captures the metal-containing raw material from the process gas; and A heating unit heats the collecting unit according to the viscosity of the metal-containing raw material.

2. The raw material capture system according to claim 1, characterized in that: The raw material collection system further comprises: a storage unit for recovering the metal-containing raw material; The metal-containing raw material in the collecting portion is heated by the heating portion and recovered to the storage portion.

3. The raw material capture system according to claim 1, characterized in that: The raw material collection system further comprises: a pump, which is provided between the processing chamber and the first exhaust line in the exhaust pipe and performs vacuum exhaust on the processing gas. The collecting portion is disposed on the secondary side of the pump.

4. The raw material capture system according to claim 1, characterized in that: The collecting portion is configured so that the metal-containing raw material does not undergo phase change due to heating by the heating portion.

5. The raw material capture system according to claim 1, characterized in that: The raw material collection system comprises: a cooling part for cooling the collection part; The cooling unit is configured to cool the processing gas flowing into the collecting unit.

6. The raw material capture system according to claim 2, characterized in that: The raw material collection system comprises: a connecting portion connecting the collecting portion and the storage portion; The connecting portion is configured to inhibit the metal-containing raw material from adhering to the side wall of the storage portion.

7. The raw material capture system according to claim 6, characterized in that: The collecting portion includes a guide portion configured to guide the metal-containing raw material toward the bottom of the storage portion.

8. The raw material capture system according to claim 1, characterized in that: The raw material collecting system is configured to adjust the heating of the collecting portion by the heating portion so that the metal-containing raw material has a viscosity that allows it to flow in the collecting portion in the direction of gravity.

9. The raw material capture system according to claim 1, characterized in that: A first valve is provided on the upstream side of the collecting portion in the first exhaust line, A second valve is provided on the downstream side of the collecting portion in the first exhaust line, The raw material collection system is configured such that the collection portion can be disconnected from the first exhaust line by closing the first valve and the second valve.

10. The raw material capture system according to claim 1, wherein: The raw material collecting system is configured to supply the heat medium flowing through the heating portion from the lower side toward the upper side of the collecting portion.

11. The raw material capture system according to claim 5, characterized in that: The raw material collecting system is configured to supply the heat medium flowing through the cooling portion from the lower side toward the upper side of the collecting portion.

12. The raw material capture system according to claim 3, characterized in that: The raw material collection system further comprises: a detoxification device, which is arranged in the exhaust pipe at a position downstream of the collecting portion and detoxifies the processed gas. The raw material collection system is configured to be capable of heating the exhaust pipe from the pump to the abatement device.

13. The raw material capture system according to claim 3, characterized in that: The raw material collection system is provided with: a second exhaust line provided in the exhaust pipe so as to bypass the first exhaust line; and a harm removal device for removing harm from the treated gas flowing through the exhaust pipe, The raw material collection system is configured to be capable of heating the entire pipe extending from the pump through the second exhaust line to the abatement device.

14. The raw material capture system according to claim 2, wherein: By connecting the ports of the T-branch pipe facing each other, the collecting part and the storage part are connected linearly. The processing gas is discharged from a port of the T-branch pipe that does not face the port.

15. The raw material capture system according to claim 9, wherein: The first valve includes a first automatic valve and a first manual valve, wherein the first manual valve is disposed downstream of the first automatic valve. The second valve includes a second automatic valve and a second manual valve, wherein the second manual valve is provided upstream of the second automatic valve. A first detachable portion is provided between the first automatic valve and the first manual valve. A second detachable portion is provided between the second automatic valve and the second manual valve.

16. The raw material capture system according to claim 2, wherein: The inlet of the processing gas is provided at the upper end of the collecting portion, The outlet of the processing gas is provided at the lower end of the collecting portion, The process gas flows downward inside the collecting portion from the inlet to the outlet, The metal-containing raw material is dripped from the outlet into the storage portion.

17. The raw material capture system according to claim 16, wherein: The collecting part is cooled by a refrigerant. A gas contact surface for agglomerating the metal-containing raw material is formed on a vertical surface in the collecting portion.

18. The raw material capture system according to claim 1, wherein: The temperature of the heating unit is set so that the viscosity of the metal-containing raw material is not more than a predetermined viscosity and the vapor pressure is not more than a predetermined pressure.

19. A substrate processing device, characterized in that: have: a processing chamber for processing a substrate disposed therein; a metal-containing gas supply system for supplying a process gas containing a metal-containing raw material into the process chamber; and a raw material capture system that captures the metal-containing raw material from the process gas exhausted from the process chamber by a pump, The raw material capture system has: an exhaust pipe for guiding the discharged processed gas; a collecting portion, which is provided in the first exhaust line constituting the exhaust pipe and recovers the metal-containing raw material from the processed gas; and A heating unit heats the collecting unit according to the viscosity of the metal-containing raw material.

20. A method for capturing raw materials, characterized in that: Has the following processes: exhausting the process gas containing the metal-containing raw material from the process chamber through an exhaust pipe; A collecting portion provided in a first exhaust line constituting the exhaust pipe captures the metal-containing raw material from the process gas; and The collecting portion is heated by a heating portion according to the viscosity of the metal-containing raw material, so that the metal-containing raw material in the collecting portion drips outward.

21. A method for manufacturing a semiconductor device, characterized in that: Has the following processes: supplying a gaseous metal-containing raw material containing a metal element into a processing chamber to form a film containing the metal element on a substrate in the processing chamber; exhausting the process gas containing the metal-containing raw material from the process chamber through an exhaust pipe; A collecting portion provided in a first exhaust line constituting the exhaust pipe captures the metal-containing raw material from the process gas; and The collecting portion is heated by a heating portion according to the viscosity of the metal-containing raw material, so that the metal-containing raw material in the collecting portion drips outward.

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